Benzenecarboximidic acid, 3-methoxy-, ethyl ester, hydrochloride → HCID 59519026, 화합물

HRID 1161855노트

반응식

HRID 1161855 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]2[CH:20]=[CH:19][C:18]([NH2:21])=[C:17]([C:22](=[O:31])[NH:23][CH2:24][C:25](=[O:30])[NH:26][CH:27]([CH3:29])[CH3:28])[CH:16]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl.[CH3:33][O:34][C:35]1[CH:36]=[C:37]([CH:43]=[CH:44][CH:45]=1)[C:38](=N)OCC>CCO>[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]2[CH:16]=[C:17]3[C:18](=[CH:19][CH:20]=2)[N:21]=[C:38]([C:37]2[CH:43]=[CH:44][CH:45]=[C:35]([O:34][CH3:33])[CH:36]=2)[N:23]([CH2:24][C:25](=[O:30])[NH:26][CH:27]([CH3:28])[CH3:29])[C:22]3=[O:31])[CH2:10][CH2:9]1)=[O:7])([CH3:2])([CH3:4])[CH3:3]

참가 물질

4

반응물 2

HCID 12282163Benzenecarboximidic acid, 3-methoxy-, ethyl ester, hydrochlorideHCID 67417372HCID 67417372, 화합물

생성물 1

HCID 59519026HCID 59519026, 화합물수율 13%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 4-{4-Amino-3-[(isopropylcarbamoylmethyl)carbamoyl]phenyl}perhydro-1,4-diazepine-1-carboxylic acid tert-butyl ester (INTERMEDIATE V.2) (300 mg, 0.69 mmol) and ethyl 3-methoxybenzimidate hydrochloride (INTERMEDIATE II.2) (298 mg, 1.38 mmol) in EtOH (6 mL) was heated at reflux temperature for 16 h. The reaction mixture was cooled, filtered and the filtrate concentrated in vacuo. The crude residue was purified by preparative HPLC to afford 4-[3-(isopropylcarbamoylmethyl)-2-(3-methoxyphenyl)-4-oxo-3,4-dihydroquinazolin-6-yl]perhydro-1,4-diazepine-1-carboxylic acid tert-butyl ester (INTERMEDIATE VII.1) (50 mg, 0.09 mmol, 13%).

후처리

  1. temperaturewas heated
  2. temperatureat reflux temperature for 16 h
  3. temperatureThe reaction mixture was cooled
  4. filtrationfiltered
  5. concentrationthe filtrate concentrated in vacuo
  6. customThe crude residue was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-09aeeba715524762bbccf20a604bc74f
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07820649B2

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